Persistent organic pollutants in food

Solutions for POPs in food testing

Persistent organic pollutants in food

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

Table of contents

Complete POPs in food solutions

Environmental pollutants in foods and beverages—such as persistent

organic pollutants, also known as POPs—are of great interest when

it comes to food safety. Dioxins, polychlorinated biphenyls (PCBs),

organochlorine pesticides (OCPs), and polybrominated diphenyl

ethers (PBDEs) are among the most common. Other chemicals

including fluorinated substances, chlorinated naphthalenes,

pentachlorophenol, and chlorinated paraffins are in various stages

of becoming officially designated as POPs.

Dioxins in food, such as polychlorinated dibenzo-p-dioxins (PCDDs),

polychlorinated dibenzofurans (PCDFs), and polychlorinated

biphenyls (PCBs), constitute a group of highly toxic organic

compounds formed unintentionally, mainly in waste combustion

processes or as by-products of industrial manufacturing of certain

chemicals, such as chlorinated pesticides.

Resistant to environmental degradation, POPs bioaccumulate up the

food chain and often occur as residues in fatty foods including meat,

fish, eggs, or other dairy products. They can have significant effects

on humans and animals as they migrate through the food chain. The

EU has demanding regulatory limits for OCPs, PCBs, and PCDDs/

PCDFs in animal feed and animal and fish products for human

consumption.

More information on POPs, from improvements in instrumentation

and methods, drive the need for ever-lower limits of detection and

quantitation, for both known and unknown compounds. Using

state-of-the-art high-resolution mass spectrometry (HRMS), we

provide solutions for some of the most challenging food safety and

environmental pollutant determinations.

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

Table of contents

The Thermo Scientific™ Dionex™ ASE™ 350 Accelerated Solvent

Extraction system is used for the extraction of organic pollutants

from solid and semisolid samples. This system is suitable for

extraction of pollutants from high-fat content and dry foods

such as avocados and tea. The Dionex ASE system is

equivalent to or better than Soxhlet, automated Soxhlet,

sonication, and shaking techniques.

Use of the novel water-absorbing polymer Thermo Scientific™

Dionex™ ASE Prep MAP dispersant and sorbent expands the

capabilities of the accelerated solvent extraction technique and

allows for the extraction of analytes from samples containing up to

85% water.

Thermo Scientific Dionex ASE 350 Accelerated Solvent Extractor system

Learn more

Accelerated solvent extraction

Accelerated solvent extraction

Table of contents

Complete POPs in food solutions

Dioxins in oysters

POPs in fish tissue

DFS GC-HRMS

GC and GC-MS

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

Techniques such as Soxhlet and sonication are used for the

extraction of halogenated hydrocarbons from food and

environmental samples prior to their analytical determination.

These techniques are, however, very labor intensive and suffer

from high solvent consumption. The accelerated solvent extraction

technique meets the new requirements of increased throughput

and reduced solvent usage in sample preparation as extractions

can be completed quickly using minimal solvent. Recent advances

using accelerated solvent extraction systems, as described in

several publications,1-19 include procedures for selective removal of

interferences during sample extraction, thus combining extraction

and purification into a single step. The method reported here is

applicable for the determination of 29 halogenated hydrocarbons

(6 PCBs, 16 OCPs, and 7 PBDEs) in fish tissues. Detection via MS/

MS provides both quantitative information and confirmation of POP

residues in tuna, substantiating that the one-step accelerated solvent

extraction method is a valid faster alternative to classic extraction

methods because the analytical quality is comparable.

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Table of Contents

POPs in fish tissue

Total ion current (GC-MS/MS) chromatogram of tuna spiked sample.

Dioxins in oysters

POPs in fish tissue

Complete POPs in food solutions

Accelerated solvent extraction

Table of contents

DFS GC-HRMS

GC and GC-MS

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

Dioxins in oysters

Accelerated solvent extraction is a high-temperature, high-pressure

extraction technique that is widely used for sample extractions in the

environmental, chemical, and food analysis industries. Extractions at

higher temperatures and pressures allow faster extraction of analytes

relative to conventional solid-liquid-based extraction techniques

such as Soxhlet. Spiked oyster samples were either treated with

Dionex ASE Prep MAP and Dionex ASE Prep DE (1:1) or by using

sodium sulfate as the drying agent prior to in-cell extraction in the

Dionex ASE 350 system. The data shows that Dionex ASE Prep

DE is an effective drying agent for wet oyster samples with excellent

recoveries for the six OCPs.

Download the poster note

In-cell moisture removal of oyster sample using Dionex ASE Prep MAP and Dionex ASE Prep DE

* Data is courtesy of Department of Toxicology, Texas Tech University, Lubbock, TX, USA** In-cell drying with sodium sulfate is not recommended using the ASE instrument

Dioxins in oysters

% Recovery oyster dried with

Dionex ASE Prep MAP and Dionex ASE Prep DE*

% Recovery oyster dried with sodium sulfate**

Compound (n = 3) (n = 3)

Lindane 91 81

Heptachlor 93 64

Aldrin 94 66

Dieldrin 105 75

Endrin 106 70

DDT 114 69

Total 101 71

POPs in fish tissue

Complete POPs in food solutions

Accelerated solvent extraction

Table of contents

DFS GC-HRMS

GC and GC-MS

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

Achieve outstanding sensitivity for analysis of dioxins and

persistent organic pollutants in food with the Thermo Scientific™

DFS™ Magnetic Sector GC-HRMS system. The DFS GC-HRMS

system with double-focusing delivers ultimate mass spectrometry

performance for target compound analysis. It also offers worldwide

full compliance with any official dioxin, PCB, or PBDE method (for

example, EPA 1613, 1668, or 1614). Exploit the benefits of the

highest available dioxin sensitivity and robustness, delivered by our

large-volume ion source. A product of 50 years of experience in

developing magnetic sector MS, the DFS GC-HRMS system has all

the features you need for your food applications.

DFS™ Magnetic Sector GC-HRMS systemLearn more

DFS GC-HRMS

DFS GC-HRMS

Complete POPs in food solutions

Accelerated solvent extraction

Table of contents

Analysis of polychlorinated dioxins/furans

GC and GC-MS

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

Magnetic sector high-resolution GC-MS is the gold standard for

high sensitivity analysis of dioxins and other POPs. For decades

it has proven its proficiency in this field of analysis and thus has

become the established analysis technique available in leading dioxin

laboratories throughout the world. The analytical performance with

the DualData XL Acquisition configuration and conventional GC-MS

configuration was compared using the same set of polychlorinated

dioxins and furans, PCBs, and PBDE samples as model compounds.

Download the technical note

Analysis of polychlorinated dioxins/furans

Example of peak integrity of dioxin trace analysis (Hexa CDD/F) using the DualData XL Acquisition configuration.

Analysis of polychlorinated dioxins/furans

Complete POPs in food solutions

Accelerated solvent extraction

Table of contents

GC and GC-MS

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

DFS GC-HRMS

GC and GC-MS

Meet your stringent requirements for performance, reliability,

and value with Thermo Scientific™ gas chromatography-mass

spectrometer (GC-MS) systems. Combine powerful GC-MS

instruments with productivity-enhancing software to create complete

solutions for the most challenging POPs testing. Achieve analysis of

dioxins in food and feed and meet demanding performance criteria.

GC instruments from Thermo Fisher Scientific provide outstanding

performance for routine analyses, advanced capabilities, and the

flexibility to increase sample throughput. Instant-connect injectors

and detectors enable you to change modules in minutes to

reconfigure the instrument for new workflows, develop new methods,

and eliminate maintenance downtime. Current developments in

GC-MS triple quadrupole technology deliver high sensitivity and

selectivity in the small molecule mass range and allow the detection

of compounds at low concentrations, even in complex matrix

samples. A simple and standard approach using electron impact

ionization (EI) enables a very straightforward method for low-level

analysis.

Learn more

GC and GC-MS

Thermo Scientific™ TSQ™ 8000 Evo Triple Quadrupole GC-MS/MS system

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

Table of contents

Dioxin-like PCBs in food and feed

POPs in honey

PCDD/Fs in food and feed samples

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

Polychlorinated biphenyls (PCBs) are a group of highly toxic

organochlorine compounds with 209 possible congeners, depending

on the number and position of the chlorine atoms. These congeners

can be divided into two groups based on their structural and

toxicological characteristics. The first group comprises 12 congeners

that have a structure and toxicity similar to dioxins. These are

termed “dioxin-like PCBs” (DL-PCBs) and are the focus of this

study. The other group, forming the majority, do not exhibit the

same degree of toxicity and these are called “non-dioxin-like PCBs”

(NDL-PCBs). The potential for human exposure to these compounds

makes accurate detection and quantification of DL-PCBs in the

environment, particularly in food and animal feed, very important. The

instrumental method used was based on that described in previous

work analyzing PCDD/Fs using GC-MS/MS. The results obtained

demonstrate that GC-MS/MS is a highly sensitive and selective

analytical system that can be confidently used for DL-PCB

detection and confirmation in food and feed samples.

Download the poster note

Dioxin-like PCBs in food and feed

Example of chromatographic separation of the pentachlorobiphenyl congeners in the CS-1 standard (1 pg/µL).

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Dioxin-like PCBs in food and feed

POPs in honey

PCDD/Fs in food and feed samples

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

Table of contents

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

Honey is a natural product that is widely used for both nutritional and

medicinal purposes. It is generally considered a natural and healthy

product of animal origin and free of impurities. Consumer preference

for natural products and the demand for quality ingredients and

clean-label products, including organic honey, is increasing.

Many pollutants in the environment can contaminate the bees

themselves in addition to their pollen, honey, and other bee products.

Environmental pollutants include pesticides, heavy metals, bacteria,

and radioactive materials. Among the environmental contaminants,

studies have documented the occurrence of organochlorines

(OCs), polychlorobiphenyls (PCBs), organophosphates (OPs),

and polybromodiphenylethers (PBDEs) in honey. The European

Commission has set the maximum residue level values (MRLs) for

feed as well as for food of animal origin for these chemicals. The

method reported here is applicable for the determination of four

different classes of compounds (6 PCBs, 7 PBDEs, 16 OCs, and

19 OPs) in honey. Eleven additional compounds, belonging to

different classes and commonly used as agrochemicals, have

also been investigated.

Download the application note

Distribution of detected contaminants (ng/g) in organic honey samples according to their sampling area.

POPs in honey

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PC

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PC

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Hep

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South Italy (Calabria)

North Italy (Trentino)

North Italy (Lombardia)

*

*

Dioxin-like PCBs in food and feed

POPs in honey

PCDD/Fs in food and feed samples

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

Table of contents

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

Legislation in the European Union previously required the

confirmation and quantification of PCDD/Fs in contaminated

samples by gas chromatography/high-resolution mass spectrometry

(GC-HRMS) instruments, considered the “gold standard” approach.

However, technological advances in gas chromatography/triple-

quadrupole mass spectrometry (GC-MS/MS) technology allowed

high sensitivity and selectivity to be achieved. These improvements

have led to GC-MS/MS being considered a reliable tool that can be

used to control the maximum levels for PCDD/Fs in food and feed

as a full confirmatory method. The dioxin content of each sample,

expressed as WHO-PCDD/F-TEQ pg/g, was determined for each

sample analyzed, and the results were compared with the existing

data obtained for the same samples from the GC-HRMS. The

calculated concentrations of each individual PCDD/F congener

(as TEQ pg/g) were compared with the values obtained from the

GC-HRMS. The data shows excellent agreement.

Download the application note

PCDD/Fs in food and feed samples

PCDD/Fs in food and feed samples

GC-HRMS

GC-MS/MS

Individual contribution of each PCDD/F congener to the feed sample dioxin content (as TEQ pg/g) and comparison of Thermo Scientific™ TSQ™ 8000 Evo GC-MS/MS system results with the GC-HRMS values.

Dioxin-like PCBs in food and feed

POPs in honey

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

Table of contents

GC-HRAM

LC-MS

LC-HRAM

Peer reviewed journals

GC-HRAM

Bring the power of the first-ever combination of high-resolution

gas chromatography (GC) and high-resolution, accurate-mass

(HRAM) Orbitrap™ mass spectrometry to your laboratory. The

Thermo Scientific™ Q Exactive™ GC Orbitrap™ GC-MS/MS system

provides comprehensive characterization of samples in a single

analysis for the highest confidence in compound discovery,

identification, and quantitation. This system offers the quantitative

power of a GC triple quadrupole MS combined with the high-

precision, full-scan HRAM capabilities only available in combination

with Thermo Scientific™ Orbitrap™ technology.

The Thermo Scientific™ Exactive™ GC Orbitrap™ GC-MS system is

the first-ever combination of high-resolution gas chromatography and

high-resolution, accurate-mass (HRAM) Orbitrap mass spectrometer.

It is an easy-to-use, dedicated benchtop GC-MS system that provides

the highest confidence for emerging POPs research with unmatched

performance in compound discovery, identification, and quantitation

for a comprehensive understanding of your samples.

Learn more

GC-HRAM

Thermo Scientific™ Q Exactive™ GC Orbitrap™ GC-MS/MS system

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

Table of contents

LC-MS

LC-HRAM

Peer reviewed journals

Short-chained chlorinated paraffins

Identification of novel brominated flame retardants

Short-chained chlorinated paraffins

Short-chained chlorinated paraffins (SCCPs) are emerging

contaminants that, once released, remain in the environment for

long periods with the potential to bio-accumulate in living organisms.

Detection and quantification of SCCPs pose analytical challenges

due to the fact that these compounds are present in the environment

at low levels, as very complex isomeric mixtures, and are difficult to

separate chromatographically. Complete separation of SCCPs is

also challenging because of the very high numbers of isomers and

homologues with similar physiochemical properties. In this study,

the performance of a novel benchtop high-resolution, accurate-

mass Orbitrap™-based GC-MS was tested for the analysis of

SCCPs. The Thermo Scientific™ Exactive™ GC Orbitrap™ GC-MS

system is a potential solution to the difficult challenges related to the

detection and quantification of SCCPs due to its excellent sensitivity,

linearity, and selectivity and in combination with its uncomplicated

instrumental setup.High-resolution, accurate-mass selectivity demonstrated for the C10-C13 63% technical mix acquired in NCI at 60k resolution. Examples of extracted ion chromatograms for individual homologues with various chlorination degrees are shown.

Download the technical note

C10H15Cl6

C11H17Cl6

10.15 C11H16Cl7

10.73 C12H18Cl7

10.69

11.21

10.22

11.70

9.72

RT: 6.48 - 14.43

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NL: 2.00E8 TIC MS

NL: 2.00E7 m/z= 346.92652

NL: 3.00E7 m/z= 360.94208

NL: 3.00E7 m/z= 394.90330

NL: 2.00E7 m/z= 408.91872

NL: 2.00E7 m/z= 444.87597

NL: 2.00E7 m/z= 458.89157

NL: 2.00E7 m/z= 492.85283

TIC

11.20 C12H17Cl8

11.73 C13H19Cl8

C13H18Cl9

Short-chained chlorinated paraffins

Identification of novel brominated flame retardants

GC-HRAM

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

Table of contents

LC-MS

LC-HRAM

Peer reviewed journals

Due to legislative restrictions on the manufacture and use of some

brominated flame retardants (BFRs), several new chemicals (NBFRs)

have been developed. To explore their presence in different food

and environmental compartments, and ultimately understand their

environmental fate, analytical methods for targeted analysis are

required. Classically, these compounds are determined by GC-

based instrumental methods. In recent years, LC-based methods

coupled to low-resolution mass spectrometers have also been

developed. Advances in high-resolution mass spectrometry facilitate

accurate measurements and identification of unknowns, including

degradation and transformation products. Several legacy BFRs and

NBFRs were identified in dust samples. This indicates the relevance

of dust-containing chemicals as an entry pathway to human and

environmental exposure. Mass defect plots are a useful technique

to simplify any chosen mass spectrum greatly. Thermo Scientific™

Compound Discoverer™ software is a powerful tool for unknown

screening and structural identification of compounds in food and

environmental sciences.

Identification of novel brominated flame retardants

Identification of novel brominated flame retardants

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Selected (N)BFRs in dust sample.

Compounds: (2-ethylhexyltetrabromobenzoate (EH-TBB), bis(2-ethylhexyl)tetrabromophtalate (BEH-TBP), decabromodiphenyl ethane (DBDPE), tetrabrombisphenol A (TBBP-A), hexabromcyclododecane (HBCD)

Suspect compound

FormulaQuasi-molecular ion

and m/zΔ m/z (ppm)

Time (min)

EH-TBB C15H18Br4O2 [M-Br+O]- 484.87706 0.08 10.24

BEH-TBP C24H34Br4O4 [M-C8H17+H-Br]- 512.87402 0.98 11.16

DBDPE C14H4Br10 [M-Br+O]- 906.28362 0.82 12.06

TBBP-A C15H12Br4O2 [M-H]- 542.74571 0.09 8.30

HBCD C12H18Br6 [M-H]- 640.63746 0.23 9.02

Short-chained chlorinated paraffins

GC-HRAM

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

Table of contents

LC-MS

LC-HRAM

Peer reviewed journals

LC-MS

MS detection has become more affordable, accessible, and even

mandatory in many fields of research. Simply detecting a peak is

no longer sufficient; today it is necessary to know the identity of

the compound causing the response, often in accordance with

internationally accepted criteria. When our pioneering Thermo

Scientific™ Vanquish™ UHPLC platform is combined with our

best-in-class mass spectrometers, you achieve an extra level

of confidence.

The Thermo Scientific™ TSQ Altis™ and TSQ Quantis™ triple

quadrupole mass spectrometers are the perfect match for a

wide range of quantitation workflows that utilize selected reaction

monitoring (SRM) analyses.

Vanquish UHPLC and TSQ Altis triple quadrupole mass spectrometerLearn more

LC-MS

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

GC-HRAM

Table of contents

Perfluorinated compounds in human breast milk

LC-HRAM

Peer reviewed journals

Perfluorinated compounds in human breast milk

Perfluorinated compounds (PFCs) are ubiquitous and persistent

pollutants that bioaccumulate in animals and humans. The potential

toxicity of these chemicals has fueled efforts to develop robust

analytical techniques for measuring low levels of PFCs in human

matrices. Quantitative selected reaction monitoring (SRM) assays

were developed for six PFCs. PFCs were accurately and reproducibly

detected at ppt concentration in neat solution and human milk

matrix. Exceptionally sensitive and accurate, this integrated LC-MS

platform is ideally suited for robust ultra-trace analysis of PFCs in a

wide range of matrices.

The separation and detection of the PFCs in human milk matricies.

Perfluorinated compounds in human breast milk

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Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

GC-HRAM

LC-MS

Table of contents

LC-HRAM

Peer reviewed journals

Identify and confirm more compounds rapidly and with confidence.

The Thermo Scientific™ Vanquish™ UHPLC platform is a great

match for our unique Orbitrap™ technologies including the Thermo

Scientific™ Exactive™ line of benchtop mass spectrometers.

Take full advantage of all the benefits of high-resolution, accurate-

mass detection by LC-MS to identify, characterize, and quantify

unknown and known compounds within complex matrices.

Learn more

LC-HRAM

LC-HRAM

Vanquish UHPLC and Q Exactive Focus LC-MS system

Complete POPs in food solutions

Accelerated solvent extraction

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GC and GC-MS

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Find out more at www.thermofisher.com/food-safety

For Research Use Only. Not for use in diagnostic procedures. © 2017 Thermo Fisher Scientific Inc. All rights reserved. DART is a registered trademark of JEOL USA, Inc. All other trademarks are the property of Thermo Fisher Scientific and its subsidiaries unless otherwise specified. AN72422-EN 0219S

Peer reviewed journal articles:GC-MS methodsTitle Authors Publication

Meeting the European Commission performance criteria for the use of triple quadrupole GC-MS/MS as a confirmatory method for PCDD/Fs and dl-PCBs in food and feed samples

Manuela Ábalos, Cristian I. Cojocariu, Paul Silcock, Dominic Roberts, Diana M. Pemberthy, Jordi Sauló, Esteban Abad

Analytical and Bioanalytical Chemistry May 2016, Volume 408, Issue 13, Pages 3511–3525

Dibenzo-p-dioxins and dibenzofurans in human breast milk collected in the area of Taranto (Southern Italy): first case study

Giuliana Bianco, Rosalia Zianni, Giuseppe Anzillotta, Achille Palma, Vincenzo Vitacco, Laura Scrano, Tommaso R. I. Cataldi

Analytical and Bioanalytical Chemistry March 2013, Volume 405, Issue 7, Pages 2405–2410

Survey of persistent organochlorine contaminants (PCDD, PCDF, and PCB) in fish collected from the polish baltic fishing areas

Jadwiga Piskorska-Pliszczynska, Sebastian Maszewski, Malgorzata Warenik-Bany, Szczepan Mikolajczyk, and Lukasz Goraj

The Scientific World Journal Volume 2012 (2012), Article ID 973292, 7 Pages

PCDD and PCDF levels in paper with food contact H. Beck, A. Droß, W. Mathar

Chemosphere Volume 25, Issues 7–10, October–November 1992, Pages 1533–1538

Peer reviewed journal articles

Peer reviewed journals

Complete POPs in food solutions

Accelerated solvent extraction

DFS GC-HRMS

GC and GC-MS

GC-HRAM

LC-MS

LC-HRAM

Table of contents